Amedee



UNITED STATES PATENT OFFICE.

AMEDEE J. LANFREY, OF CHARTERS, FRANCE.

MANUFACTURE OF EXPLOSlVE COMPOUNDS.

SPECIFICATION forming part of Letters Patent No. 276,833, dated May 1, 1883.

Application tiled June 9,1579. Patented in France August 7, 1875, No. 3,119; in Italy August 17, 1878;

June 12, 1878, No. 124,789; in Belgium August a. Fir, No. 4935K; in

in Austria April 7, 1879, No. 5,521; in Portugal Jumll, 1 T": in

England Germany January 21, 1880, No. 12,1l9, and in Sweden August 28, 1880.

To all whom 1t may concern Be it known that I, AMEDEE JosEPH LAN- FREY, of Chartres, in the Republic of France, and an officer in the French army, have made certain new and useful Improvements in the ManufactureofExplosiveCompounds,ot'which the following is a full, clear, and exact description.

The object of this invention is improvements in the manufacture of certain explosive compounds, the basis of these new explosive substances consisting of various straws, such as corn, rye, barley, oats, and buckwheat. It is manufactured as follows: The straw is submitted to a boiling operation for fifteen or sixteen hours in an alkaline solution (carbonate of soda or of potassium) weighing from 2 to 3 Baum. In this state the straw easily disintegrates, and the fatty or other soluble matters which it contained are dissolved and carried off by the water when the latteris withdrawn. The fibers are then triturated, and a perfect washing effected at the same time, either by means of a cylinder stutf-engine similar to those employed in paper-mills or by means of revolving millstones, also similar to those used in such mills. During the trituration a current of water should constantly wash the fibers. It is essential that this pulp does not retain any alkalinereaction, which is insured by adding sulphuric or hydrochloric acid in sufficient quantity that the washing-water has a slightly-acid reaction. The fibers thus triturated and prepared are, after having been perfectly dried, ready to undergo the reactions which render them explosive. To facilitate the manipulations which follow, the pulp is treated by a papermachine, and should produce asheet weighing about three hundred grams the square meter. The thickness may vary more or less. The sheet thus formed is out, either by hand by the aid of special tools, or mechanically, into little pieces of three to four millimeters square. 4 These little pieces or fragments are then immersed for three or four hours in an acid compound composed of three volumes of smoking (t'umant azotic acid (at 46 to 48) and seven volumes of concentrated sulphuric acid, (at 66 then withdrawn from the acid bath, drained as much as possible, pressed, and finally well washed with water until there remains no trace of acid. Any acid reaction is prevented by adding to the last washingwater a little carbonate of potassium or of soda, and a'little of this alkaline water is leit in contact with the little pieces or fragments for several hours. The fragments may be immersed in a compound of nitrate of soda or potassium and concentrated sulphuric acid for their more economic transformation into nitrocellulose, the result being the same.

The object of making the sheets into fragments is to facilitate the action oi. the acids, and this result might, it is obvious, be obtained by punching holes in the sheet. In this case the acid may be pressed from the the sheet by valves which are not acted upon by the acids. It is preferable to repeat the immersion in the acids and the GXDlBiSlOll of the portion absorbed.

The nitro-cellulose. thus obtained has peculiar properties which fit it for use as an agent for blasting or use in fire-arms independentol' the quality of exploding which it has in .connection with all other kinds ot'nitro-ccllulosc. These properties are as follows:

First, stability and resistance to shocks, the inertia being in proportion to thcconta-ined silica. From analysis by Sprengel, oat-straw is found to contain 4.59 per cent., wheat 2.87 per cent., and the other straws still somewhat less, barley being 2.86 per cent. and rye 2.30 per cent.

Second, regularity of explosion and less rapid deflagration in tire-arms, due to silica.

Third, ability to obtain a weak nitrification, together with a product of homogeneous constitution, for employment in firearms, in which the combustion should be slow, progressive,and regular. Pure celluloseis nitrated too strongly, or, if the immersion in the acid bath has been for a very short time, one part is strongly nitrated and another notat all, so that a mixture is formed of cellulose and nit-ro-cellulose. In other words, the constitution is not homogeneous. Straw cellulose,which m ay be regarded as formed of pure cellulose and silica, in consequence of the presence of the latter in intimate contact therewith, is nitrated l'eebly .lose from these materials differs in itself different from and regularly even after a contact with the acids long enough for them to penetrate the entire mass. By feeble nitrification is to be understood that which produces nitrocellulose, and not trinitro-cellnlose. Nitro-ccllulose from straw satisfies, therefore, the condition mentionedto wit, it is nitrated feebly, so that the combustion is slow. and progressive, and is of a homogeneous constitution, which gives regularity to the explosion.

Fourth, :a power of absorption, which ex-- ists in a higher degreein this material than in intro-cellulose from wood or cotton. It is well known that cellulose exists in many forms from the hard shell of the seed of the plum or cherry to young sprouts, and the nitro-cellulike manner. Nitrocellulose from straw can absorb seventy-five per cent. ofnitro-glycerine,which is not possible with ordinary gun cotton or nitrated wood. Nitro-cellulose from straw is that obtained from bamboo or cane, and the process applicable to its manufacture could not be employed for the nitration of bamboo. Theeomposition of hamboo is diti'erent from straw, and their nitrated products diifer in like manner; The capacity for separation, consistency, and absorbing power is entirely different. The cellulose in cane and bamboo resembles that of wood more than straw, their rigidity being due to a large formed into paper,

quantity of incrustating material called lignine, (a matter which is very diflicult to re- 1nove,)and not to the presence of silica,which is contained in very small quantity. Moreover, straw-is an article found universally in civilized nations, while bamboo is only encountered over limited areas. The production of nitrocellulose from straw is also more economical than from other materials, such as cotton, flax, bamboo, or the like.

Having thus explained the special properties of straw nitrocellulose, the description of the process is continued as follows: 7

N itro-cellulose prepared accordingxto this invention has been kept for upward of three years without suffering any deterioration nor Solution of n iter 1 Explosive for blastin purposes.

Nte '1 Nte b bolntmn containing.

Explosive for shootil purposes.

Dextrine .At 6 to 7 Baums Niter l Hard-wood charcoal E 5 Solution containing. Dextrine iHard-wood charcoal i f i r Hard-wood charcoal 15 At 8 to 9 Bmnn E Dextrine 1 1 Hard-wood charcoal Niter t Hard-wood charcoal 20 At 16 to 17 Baum. Explosive for cannon or ordnance.

losing any of its explosive force, nor has any accident occurred resulting from spontaneous ignition during the numerous experiments to which it has been subjected. The cause of this stability (of such great importance in explosive bodies.) is the following: The straw fibers are formed of cellulose containing, when in a combined state, a considerable quantity of silica in the form of silicates: This silica in straw nitrocellulose plays a part analogous to that which it fulfills in dynamite, in which it fixes the nitro-glycerine and imparts an amount of stability to that substance which it does not possess when alone. For this reason preference is given to wheat-straw for the present process in consequence of its containing more silica than other strawsyalthough they may, however, produce good results.

The novelty of the chemical reaction of the azotic acid on-vegetable fibers is not claimed, as this has been known more than thirty years; but what is claimed is the novelty of the product obtained from a disintegrated and purified raw material which has never before been availed of for this purpose. This production is not gun-paper, because thestraw fibers purified as above described would produce exactly the same explosive without being previously transwhich is only to facilitate thesubseqnentoperations. (Jonsiderableeconotny resulting from the employment of this raw material is another advantage which is claimed for this invention. These pieces of straw nitro-cellulose thus neutralized, but retaining a slight alkaline reaction, are placed, after having been drained, into a solution of niter containing dextrine, and sometimes powdered charcoal, in a state of suspension in the liquid.

The solutions, which are also claimed as part of the invention, vary according to the uses for which the explosives are required.

The following is a table of the average proportions of the substances which they should contain for obtaining explosive products with a basis of straw nitro-cellulose, and having various propertiesi (Rock or hard stone. aerometer. 5

At 6 to 7 Baums aerometer.

At 6 to 7 Baums aerometcr.

Soft stone and earth. 100 W'ood.

Explosive for sporting purposes. 15

"0 At 12 to 14 Balun. Explosive for ritlcs. 10 100 nitro-cellulose with nitro-glycerine is also claimed. It is formed as follows: The nitrocellulose is crushed in contact with two per cent. ofcarbonate of soda or of potassium under the action of revolving millstones or ofl stampers. In this operation the nitro-cellulose must contain twenty to thirty per cent. of moisture. The operationis continued until the mass appears to be nearly reduced to a powder, after which the mixture with nitro-glycerine may be made either by drying the nitro-cellulose or mixing them in a moist state and afterward dried. The proportions of nitro-glycerine to be introduced vary according to the use for which they are required. They may be from one to seventy-five per cent. In the proportion of fifty per cent., any exudation is impossible under a great pressure, and the force of this dynamite is very considerable, as may be seen by the following figures, compared with those of dynamite having an inert basis, and with pure nitro-glyeerine: Two grams of explosive substance placed in holes 0.01 meter in diameter by 0.08 meter long in cylindrical blocks of lead and filled up with water prod need, by Nobels No. 1 dynamite, containing seventy-five per cent. of nitro-glycerine; straw dynamite, or paleine, containing fifty percentofnitro-glycerine; purenitro-glycerine. Ten to fifteen per cent. of saltpeter may be added to the nitrocellulose by way of economy; but the explosive force is not increased thereby, the oxygen in excess ofthe nitro-glycerine being sutficient to combine all the free carbon of the intro-cellulose. This combination explains the large quantity of gas produced by straw dynamite or paleine.

The advantages of this compound over guncotton d y namites are, first, a greater physical stability, inertia, resistance to the mechanical action of concussions or detonating bodies by reason of the silicate in combination in the straw, consequently greater safety in its employment; secondly, considerable economy.

This straw dynamite or paleine, like guncotton dynamite, does not freeze, and easily explodes at. a very low temperature. It always retains its plasticity.

Explosives of various compositions may be manufactured by varying the proportions of the substances employed.

Having now described the nature of the said invention and in what manner the same is to be performed, I declare that I claim 1. The improved process of manufacturing nitro-cellulose by means of straw disintegrated, triturated, washed, treated with acid, and then washed and disacidulated, as before described.

2. The process of manufacturing nitro-cellulose from straw, consisting in disintegrating and otherwise preparing the straw fiber, as before set forth, forming sheets or leaves from said fiber, and then treating the paper or leaves with acids to convert the cellulose into nitrocellulose, substantially as described.

3. Nitrocellulose from straw, substantially as described, the same being in the form of paper or in other suitable form, substantially as described.

4. An explosive composition for blasting or shooting purposes, consisting of nitro-cellulosc from straw and explosive or oxidating substances, as specified, such as nitro-glycerine, niter, or mixtures of niter and carbonaceous matter, as set forth.

In testimony whereofI have signed my name to this specification before two subscribing witnesses.

A. LANFREY.

Witnesses L. RENARD, CHARLES MARDELET. 

